CN101714427A - Eu(III)-1,10 phenanthroline complex/carbon nanotube conducting fluorescence composite material and preparation method thereof - Google Patents
Eu(III)-1,10 phenanthroline complex/carbon nanotube conducting fluorescence composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides an Eu(III)-1,10 phenanthroline complex/carbon nanotube novel conducting fluorescence composite material. Eu(III)-1,10 phenanthroline complexes are uniformly dispersed on the surface of a carbon nanotube, and the carbon nanotube is completely coated. The Eu(III)-1,10 phenanthroline complexes are uniformly coated on the surface of the carbon nanotube by the adsorbing performance of the carbon nanotube and an ultraphonic dispersion technology, and the problem of compounding of the Eu(III)-1,10 phenanthroline complexes and the carbon nanotube is solved; on the premise of not influencing the conducting performance of the carbon nanotube, the composite material has certain fluorescence performance and is mainly applied to the fields of conduction, fluorescence, sensors, and the like.
Description
Technical field
The invention belongs to technical field of composite materials, relate to a kind of conductive nano, fluorescence composite material, relate in particular to a kind of based on carbon nano-tube, with Eu (III)-1,10 phenanthroline complexs are for coating outer field Eu (III)-1,10 Phen/carbon nano-tube two-phase conduction, fluorescence composite material; The present invention also relates to the preparation method of this Eu (III)-1,10 Phen/carbon nanotube conducting, fluorescence composite material simultaneously.
Background technology
The ideal structure of carbon nano-tube is seamless, the hollow tube that the former sub-grid of hexagonal carbon surrounds, and is to be formed by two-dimentional Graphene lamella convolution, and two ends are sealed by hemispheric big fullerene molecule.Carbon nano-tube becomes the focus of physics, chemistry, material science and nanosecond science and technology area research owing to accurate one dimension tubular structure and its specific structure mechanics, electricity and the chemical property of its uniqueness.Comprise the difference of the carbon atom number of plies according to tube wall, carbon nano-tube can be divided into multi-walled carbon nano-tubes (MWCNT) and Single Walled Carbon Nanotube (SWCNT).Carbon nano-tube has very high axial strength and rigidity, its mechanical property obviously is better than other crystalline materials, the seamless tubular shaped structure of the hollow of carbon nano-tube makes it have lower density and good structural stability, makes carbon nano-tube have tempting application prospect in fields such as composite material, power conversion, transducer and catalyst.
Because the existence of the quantum confined effect of electronics, the electronics in the carbon nano-tube can only be restricted its radial motion along the axial motion of nanotube in the mono-layer graphite lamella, so carbon nano-tube has unique electrical properties.Good electrical conductivity, chemical stability and light absorptive make its multi-functional nanometer material that becomes electronics or hole-transfer, are applied more and more in photoelectric conversion material and device.The nano particle of various functions is assembled in carbon nano tube surface, carbon nano-tube is modified, can prepare composite material with specific function.People such as L.Valentini are compound with carbon nano-tube and macromolecule, prepared the composite material with fluorescence property, but its technology is too complicated, also needs to use Ni-Y as catalyst, improved the cost of experiment greatly.Eu (III) is a kind of rare earth luminescent material with good fluorescence performance.Just studied Eu (TTA) as far back as Wolff in 1963
3(TTA is a TTA) fluorescence and laser property in polymethyl methacrylate started rare earth high polymer research frontier.Divalent europium Eu has also been studied in the upright cry of certain animals of Osaka, Japan university foot
2+High-molecular luminous material.The high molecular fluorescent complex of rare-earth europium can be widely used in the various luminescent materials.
Eu (III)-1,10 phenanthroline complex is a kind of good fluorescence complex, has good fluorescence property.In view of this, we are mutually compound with carbon nano-tube with Eu (III)-1,10 phenanthroline complex, have prepared Eu (III)-1, the 10 Phen/carbon nanotube conducting fluorescence composite material that possesses electric property and fluorescence property simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material.
Another object of the present invention provides the preparation method of a kind of Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material.
Eu of the present invention (III)-1, the preparation method of 10 Phens/carbon nanotube conducting fluorescence composite material is a mixed solvent with the second alcohol and water, with 1, after the dissolving of 10 Phens, adding europium nitrate solution, is 6.5～7.5 with the pH of ammoniacal liquor regulation system, 35～45 ℃ of following stirring reactions 30～60 minutes, left standstill then 6～8 hours, and obtained containing the mixed solution of Eu (III)-1,10 phenanthroline complex; Be scattered in the ethanol (95%) carbon nano-tube is ultrasonic again, add the above-mentioned Eu of containing (III)-1 then, the mixed solution of 10 phenanthroline complexs, under room temperature, stirred 20～24 hours, filter washing, drying, grinding obtains Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material; The mole of described 1,10 Phen is 1～4 times of europium nitrate; The quality of described carbon nano-tube is 1～2 times of europium nitrate quality.
In the mixed solvent of described second alcohol and water, the volume ratio of second alcohol and water is 1: 1～1: 2.
The concentration of described europium nitrate solution is 30～60mmol/L.
Filtering with microporous membrane is adopted in described filtration.
Described drying is in 50～60 ℃ of following vacuumizes.
Eu (III)-1, the 10 Phen/carbon nanotube conducting fluorescence composite material of the present invention preparation, Eu (III)-1,10 phenanthroline complex is dispersed in carbon nano tube surface, and in CNT (carbon nano-tube) is coated on fully; The mass percent of each composition is as follows in the composite material:
Eu (III)-1,10 phenanthroline complex: 40.25～65.20%, carbon nano-tube: 34.8～59.75%.
The present invention utilizes the absorption property of carbon nano-tube, adopt ultrasonic dispersion technology to make Eu (III)-1,10 phenanthroline complexs are coated on carbon nano tube surface equably, solved Eu (III)-1, the compound problem of 10 phenanthroline complexs and carbon nano-tube, and under the prerequisite that does not influence the carbon nano-tube conductive energy, make composite material possess certain fluorescent properties again.
Below Eu (III)-1, the 10 Phen/carbon nanotube conducting of the present invention's preparation, the performance of fluorescence composite material are done further to analyze.
1, electronic microscope photos
Fig. 1 is that pure nano-carbon tube amplifies 4 * 10
4Stereoscan photograph doubly.Carbon nano tube surface wherein is very smooth, does not pass through any finishing.
Fig. 2 is that Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material amplifies 4 * 10
4Stereoscan photograph doubly.We can see clearly from Fig. 2, and the surface of carbon nano-tube is significantly coated by one deck Eu (III)-1,10 phenanthroline complex even compact ground.This is because in compound process, carbon nano-tube good adsorption performance, under stirring condition, Eu (III)-1,10 phenanthroline complexs can contact with each other fully with the surface of carbon nano-tube, and evenly be adsorbed on the surface of carbon nano-tube fully, in carbon nano-tube is coated on completely.
By Fig. 1,2 as can be seen, in Eu (III)-1, the 10 Phen/carbon nanotube conducting fluorescence composite material of the present invention's preparation, Eu (III)-1,10 phenanthroline complexs are equably attached to the surface of carbon nano-tube, and in CNT (carbon nano-tube) is coated on fully.
2, fluorescence property analysis
Fig. 3 is the fluorescence emission spectrum of pure Eu (III)-1,10 phenanthroline complex, and we can see from Fig. 3, exist three characteristic peaks at 710nm, 614nm and 589nm.
Fig. 4 is the fluorescent emission spectrogram of Eu under the same terms (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material.We can see that the characteristic peak of Eu (III)-1,10 phenanthroline complex is blue shifted to 569nm and 532nm from Fig. 4.This is because in carbon nano-tube process purification process, the surface exists a large amount of outstanding keys, interacts between these outstanding keys and the Eu (III), thereby makes the characteristic peak of emission spectrum blue shift occur.Simultaneously, the emission spectrum in the compound with respect to pure Eu (III)-1,10 phenanthroline complex a little less than.This is because carbon nano-tube is a kind of good conductor, when excitation light irradiation when the composite material because the photoelectricity conversion effet of carbon nano-tube has weakened exciting light intensity, thereby caused weakening of characteristic peak in the fluorescence spectrum.This is also consistent with people's such as Qinghua Lu research conclusion.
Via the FTIR spectrum analysis, composite material has certain fluorescent properties, and the fluorescent quenching phenomenon has taken place, and this report with document is consistent, and the fluorescent quenching phenomenon is also having crucial meaning aspect the exploration of material fluorescence property.
3, thermogravimetric analysis
Fig. 5 is the TG curve of composite material, and wherein a is the TG curve of pure nano-carbon tube, and b is the TG curve of Eu (III)-1,10 Phen/carbon nano tube compound material, and c is the TG curve of pure product Eu (III)-1,10 Phen.As can be seen from Figure 5, the thermal stability of pure carbon nano-tube is best, pure product Eu (III)-1, the thermal stability of 10 Phens is the poorest, and the thermal stability of composite material is between between the two, is greatly improved with respect to the thermal stability of pure product Eu (III)-1,10 Phen.Thermal decomposition has taken place respectively at 200～350 ℃ and 350～700 ℃ in composite material, this mainly be because Eu (III)-1,10 phenanthroline complex in the decomposition of 200～250 ℃ and 350～460 ℃.
TG the analysis showed that, Eu in the composite material (III)-1,10 Phen success mutually compound with carbon nano-tube, and thermal stability is greatly improved than Eu (III)-1,10 phenanthroline complex.
4, the analysis of electric conductivity
Table 1 is different Eu (III)-1, the conductivity of the composite material of 10 phenanthroline complex content, as can be seen from the table, the conductivity of composite material mainly concentrates between 6.67～7.14S/cm, the conductive capability of composite material does not weaken because of the growth of Eu (III)-1,10 phenanthroline complex content.This mainly is owing to the conductive structure of carbon nano-tube in recombination process does not go to pot, in addition, because Eu (III)-1.10 phenanthroline complex is less with respect to the content of carbon nano-tube, do not have influence on original conduction system of carbon nano-tube, thereby kept the excellent conducting performance of carbon nano-tube.Table 1 is the influence of Eu (III)-1,10 phenanthroline complex consumption to Eu (III)-1,10 Phen/carbon nano tube compound material conductivity.
Table 1
Indulge the above, Eu (III)-1, the 10 Phen/carbon nano tube compound material of the present invention's preparation, Eu (III)-1,10 phenanthroline complex is coated on the surface of carbon nano-tube equably, and carbon nano-tube is coated on wherein completely.Composite material has kept the original electric conductivity of carbon nano-tube, and has good thermal stability, especially is significantly improved with respect to Eu (III)-1,10 phenanthroline complex.Composite material also has certain fluorescent properties simultaneously, can be applicable to fields such as conduction, fluorescence and transducer.
Description of drawings
Fig. 1 amplifies 4 * 10 for pure nano-carbon tube
4The SEM photo
Fig. 2 is Eu (III)-1,10 Phen/carbon nano tube compound material 4 * 10
4SEM photo doubly
Fig. 3 is the fluorogram of Eu (III)-1,10 phenanthroline complex
Fig. 4 is the fluorogram of Eu (III)-1,10 Phen/carbon nano-composite material
Fig. 5 is the TG curve of pure nano-carbon tube, Eu (III)-1,10 phenanthroline complex, Eu (III)-1,10 Phen/carbon nano-composite material
(a)---pure nano-carbon tube
(b)---Eu (III)-1,10 phenanthroline complex
(c)---Eu (III)-1,10 Phen/carbon nano tube compound material
Embodiment
Embodiment 1
Take by weighing adjacent luxuriant and rich with fragrance sound of vomiting quinoline 0.2g, be dissolved in the mixed solution (volume ratio of the two is 1: 1) of 5ml ethanol and water, add 30mmol/L europium nitrate solution 30ml again, regulate pH to 7 by ammoniacal liquor.Stir 30min down at 35 ℃, leave standstill 5h then, obtain containing the mixed solution of adularescent creaming Eu (III)-1,10 phenanthroline complex.
Take by weighing purified carbon nano-tube 0.5g in the 250ml round-bottomed flask, add the ethanol of 10ml 95%, place Ultrasound Instrument, ultrasonic 15min under 40KHZ, 200W makes it to mix.
The mixed solution that contains Eu (III)-1,10 phenanthroline complex of above-mentioned preparation is joined in the round-bottomed flask.At room temperature stir 20h, with the product filtering with microporous membrane, washing at 60 ℃ of following vacuum drying 24h, is ground and is obtained Eu (III)-1,10 Phen/carbon nano-composite material.
The conductance of Eu (III)-1,10 Phen/carbon nano-composite material is 7.14S/cm.
Embodiment 2
Take by weighing adjacent luxuriant and rich with fragrance sound of vomiting quinoline 0.4g, be dissolved in the mixed solution (volume ratio of the two is 1: 1) of 5ml ethanol and water, add 30mmol/L europium nitrate solution 30ml again, regulate pH to 7 by ammoniacal liquor, stir 40min down at 40 ℃, leave standstill 6h then, obtain containing the mixed solution of adularescent creaming Eu (III)-1,10 phenanthroline complex.
Take by weighing purified carbon nano-tube 0.5g in the 250ml round-bottomed flask, add the ethanol of 10ml 95%, place Ultrasound Instrument, ultrasonic 15min under 40KHZ, 200W makes it to mix.
Above-mentioned preparation contained Eu (III)-1, the mixed solution of 10 phenanthroline complexs joins in the round-bottomed flask, at room temperature stir 21h, with the product filtering with microporous membrane, washing, at 60 ℃ of following vacuum drying 24h, grind and obtain Eu (III)-1,10 Phen/carbon nano-composite material.
The conductance of Eu (III)-1,10 Phen/carbon nano-composite material is 6.67S/cm.
Embodiment 3
Take by weighing adjacent luxuriant and rich with fragrance sound of vomiting quinoline 0.6g, be dissolved in the mixed solution (volume ratio of the two is 1: 2) of 5ml ethanol and water, add 30mmol/L europium nitrate solution 30ml again, regulate pH to 7 by ammoniacal liquor, stir 50min down at 40 ℃, leave standstill 7h then, obtain containing the mixed solution of adularescent creaming Eu (III)-1,10 phenanthroline complex.
Take by weighing purified carbon nano-tube 0.5g in the 250ml round-bottomed flask, add the ethanol of 10ml 95%, place Ultrasound Instrument, ultrasonic 15min under 40KHZ, 200W makes it to mix.
Above-mentioned preparation contained Eu (III)-1, the mixed solution of 10 phenanthroline complexs joins in the round-bottomed flask, at room temperature stir 23h, with the product filtering with microporous membrane, washing, at 60 ℃ of following vacuum drying 24h, grind and obtain Eu (III)-1,10 Phen/carbon nano-composite material.
The conductance of Eu (III)-1,10 Phen/carbon nano-composite material is 6.67S/cm.
Embodiment 4
Take by weighing adjacent luxuriant and rich with fragrance sound of vomiting quinoline 0.8g, be dissolved in the mixed solution (volume ratio of the two is 1: 2) of 5ml ethanol and water, add 30mmol/L europium nitrate solution 30ml again, regulate pH to 7, wait to produce white creaming by ammoniacal liquor.Stir 60min down at 45 ℃, leave standstill 8h then, obtain containing the mixed solution of adularescent creaming Eu (III)-1,10 phenanthroline complex.
Take by weighing purified carbon nano-tube 0.5g in the 250ml round-bottomed flask, add the ethanol of 10ml 95%, place Ultrasound Instrument, ultrasonic 15min under 40KHZ, 200W makes it to mix.
Above-mentioned preparation contained Eu (III)-1, the mixed solution of 10 phenanthroline complexs joins in the round-bottomed flask, at room temperature stir 24h, with the product filtering with microporous membrane, washing, at 60 ℃ of following vacuum drying 24h, grind and obtain Eu (III)-1,10 Phen/carbon nano-composite material.
The conductance of Eu (III)-1,10 Phen/carbon nano-composite material is 7.14S/cm.
Claims (7)
1. an Eu (III)-1, the preparation method of 10 phenanthroline complexs/carbon nanotube conducting fluorescence composite material is characterized in that: with the second alcohol and water is mixed solvent, with 1, after the dissolving of 10 Phens, adding europium nitrate solution, is 6.5～7.5 with the pH of ammoniacal liquor regulation system, 35～45 ℃ of following stirring reactions 30～60 minutes, left standstill then 6～8 hours, and obtained containing the mixed solution of Eu (III)-1,10 phenanthroline complex; Be scattered in the ethanol carbon nano-tube is ultrasonic again, add the mixed solution of the above-mentioned Eu of containing (III)-1,10 phenanthroline complex then, under room temperature, stirred 20～24 hours, and filtered, washing, drying is ground and is obtained Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material; The mole of described 1,10 Phen is 1～4 times of europium nitrate; The quality of described carbon nano-tube is 1～2 times of europium nitrate quality.
According to claim 1 Eu (preparation method of (III)-1,10 Phen/carbon nanotube conducting, fluorescence composite material is characterized in that: in the mixed solvent of described second alcohol and water, the volume ratio of second alcohol and water is 1: 1～1: 2.
3. the preparation method of Eu (III)-1,10 Phen according to claim 1, it is characterized in that: the concentration of described europium nitrate solution is 30～60mmol/L.
4. the preparation method of Eu (III)-1,10 Phen according to claim 1, it is characterized in that: filtering with microporous membrane is adopted in described filtration.
5. the preparation method of Eu (III)-1,10 Phen according to claim 1 is characterized in that: described drying is in 50～60 ℃ of following vacuumizes.
6. Eu (III)-1, the 10 Phen/carbon nanotube conducting fluorescence composite material of method preparation according to claim 1.
7. as Eu (III)-1,10 Phen/carbon nanotube conducting fluorescence composite material as described in the claim 6, it is characterized in that: Eu (III)-1,10 phenanthroline complex is dispersed in carbon nano tube surface, and in CNT (carbon nano-tube) is coated on fully; The mass percent of each composition is as follows in the composite material:
Eu (III)-1,10 phenanthroline complex: 40.25～65.20%, carbon nano-tube 34.8～59.75%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102115668A (en) * | 2010-12-17 | 2011-07-06 | 西北师范大学 | Novel temperature-sensitive fluorescent nano composite material and preparation method thereof |
| CN103333345A (en) * | 2013-04-25 | 2013-10-02 | 安康学院 | Dendrimer-rear earth complex/carbon nano-tube composite material and synthesis method thereof |
| CN105154069A (en) * | 2015-09-21 | 2015-12-16 | 山东农业大学 | Multi-colored adjustable light-emitting material of nitrogen-doped carbon dot coordination rare earth and preparation method thereof |
| CN105754276A (en) * | 2016-03-25 | 2016-07-13 | 惠州学院 | Polymer film material with temperature fluorescence response and preparation method of polymer film material |
| CN108948012A (en) * | 2018-08-14 | 2018-12-07 | 苏州大学 | Lanthanide luminous material and preparation method thereof with triple luminous |
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2009
- 2009-12-08 CN CN2009101177065A patent/CN101714427B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115668A (en) * | 2010-12-17 | 2011-07-06 | 西北师范大学 | Novel temperature-sensitive fluorescent nano composite material and preparation method thereof |
| CN102115668B (en) * | 2010-12-17 | 2013-04-24 | 西北师范大学 | Novel temperature-sensitive fluorescent nano composite material and preparation method thereof |
| CN103333345A (en) * | 2013-04-25 | 2013-10-02 | 安康学院 | Dendrimer-rear earth complex/carbon nano-tube composite material and synthesis method thereof |
| CN103333345B (en) * | 2013-04-25 | 2015-11-18 | 安康学院 | Dendrimer, dendritic polymer-rare earth compounding/carbon nano tube compound material and synthetic method thereof |
| CN105154069A (en) * | 2015-09-21 | 2015-12-16 | 山东农业大学 | Multi-colored adjustable light-emitting material of nitrogen-doped carbon dot coordination rare earth and preparation method thereof |
| CN105754276A (en) * | 2016-03-25 | 2016-07-13 | 惠州学院 | Polymer film material with temperature fluorescence response and preparation method of polymer film material |
| CN108948012A (en) * | 2018-08-14 | 2018-12-07 | 苏州大学 | Lanthanide luminous material and preparation method thereof with triple luminous |
| WO2020034132A1 (en) * | 2018-08-14 | 2020-02-20 | 苏州大学 | Lanthanide luminescent material having triple luminescent channel and preparation method therefor |
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